超高效液相色谱-串联质谱法快速检测农田灌溉水中甲嘧磺隆等3种磺酰脲类农药

Determination of Three Sulfonylurea Pesticidles Including Sulfometuron-methyl in Irrigation Water by HPLC-MS/MS

建立了农田灌溉水中甲嘧磺隆等3种磺酰类农药高效液相色谱-串联质谱检测方法。灌溉水采用乙腈提取,离心振荡后无需净化,浓缩后直接过膜后上机。以甲醇和水(含0.1%甲酸)为流动相梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,外标法定量。甲嘧磺隆、苯磺隆、苄嘧磺隆在0.005~1.0 mg/L范围内线性关系良好,相关系数(r)≥0.999;3个农药回收率范围为83.8%~103.1%;变异系数范围分别为1.8%~13.1%。该方法操作简单,快速准确,满足农药残留分析要求。

A method has been established for the residue determination of three sulfonylurea pesticides,including sulfometuron-methyl,in irrigation water by liquid chromatography-tandem mass spectrometry(LC-MS/MS).The extraction of these pesticides,without purification,were achieved using acetonitrile with an oscillator by liquid-liquid partition in irrigation water.The extracted samples were directly injected into LC-MS/MS through a 0.22µm organic membrane.The analytes were separated using a mobile phase of water and methanol(containing 0.1%formic acid),detected by MS/MS with positive electrospray ionization(ESI+)in multiple reaction monitoring(MRM)mode,and quantified by external standard method.The correlation coefficient(r)for the three sulfonylurea pesticides,including sulfometuron-methyl,were found to be not lower than 0.999 within a concentration range of 0.005~1.0 mg/L.The average recoveries of these pesticides in irrigation water ranged from 83.8%~103.1%,with variation coefficients between 1.8%~13.1%.The method,characterized by its simplicity,speed,and accuracy,meets the requirements for the determination of residue analysis of pesticides.